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EPR spectroscopy is a well suited analytical tool to monitor the electronic situation around paramagnetic metal centres as copper(II) and therefore the structural influences on the paramagnetic ion. 1,2-Dithiosquaratometalates are available by direct synthesis from metal salts with dipotassium-1,2-dithiosquarate and the appropriate counter cations. Synthesis and characterisation of bis(benzyltributylammonium)1,2-dithiosquaratonickelate(II), (BzlBu 3 N) 2 [Ni(dtsq) 2 ], and bis(benzyltributylammonium)1,2-dithiosquaratocuprate(II), (BzlBu 3 N) 2 [Cu(dtsq) 2 ], with benzyltributylammonium as the counter ion is reported and the X-ray structures of two complexes, (BzlBu 3 N) 2 [Ni(dtsq) 2 ] and (BzlBu 3 N) 2 [Cu(dtsq) 2 ], are presented. Both complexes, crystallising in the monoclinic space group  P 2 1 /c, are isostructural with only small differences in the coordination sphere due to the different metal ions. The diamagnetic nickel complex is therefore well suited as a host lattice for the paramagnetic Cu(II) complex to measure EPR for additional structural information.

EPR on bis(1,2-dithiosquarato)cuprate(II) in the bis(1,2-dithiosquarato)nickelate(II) host lattice – structure and spectroscopy ‡